Hard waxes and fatty products derived from crude sugar cane waxes



Patented Aug. 7, 1945 mum WAXES Royal '1. Balch, Washington,

WAXES AND FATTY PRODUCTS DE- FROM CRUDE SUGAR CANE D. 0., assignor to Claude R. Wickard, as Secretary of Agriculture oi the United States of America, and his successors in oflice No Drawing. Application July 25, 1942,-

Serial No. 452,370

(Granted under the act of March 3, 1883, as

amended April 30, 1928; 3'70 0. G. 757) t This application is made under the act of March -3, 1883, as amended by the act of April 30, 1928,

and the invention herein described, if patented, may be manufactured and used by or forthe Government of the United States of America for governmental purposes without the p yment to me of any royalty thereon.

This invention relates to hard waxes and fatty products derived from crude suga cane waxes and to the production of them.

. Crude sugar cane waxes are extracted from clarificationmuds, or other suitable sugar cane factory waste products, by utilization of organic solvents of the waxes. The crude waxes contain many non-wax constituents orfatty portions, dependent on the variety of sugar cane from which the muds are derived, on the method by which the muds are produced in the sugar manufactur ing process, and on the solvents used for extracting the crude waxes. Some of these non-wax constituents are detrimental, if the wax is to be used industrially, and must be removed.

The object of this invention-is to utilize waste products of sugar cane factories. More specifically, the objects are crude sugar cane wax and separate fatty portions, portions into separate fractions, to produce new products, and to produce products by new processes.

into hard wax' products Preferably, the crude waxes are extracted from non-fermented materials. The clarification muds derived in the manufacture of raw sugars usually contain the higher proportions of waxes and are, therefore, the best sources from a recovery viewpoint.

It is. also preferable to dry the clarification muds at the time of their production. Theclrying should be to a point to render the muds substantially stable in the surrounding or storage atmosphere so that they may be stored without material change. This enables operation of the extraction plant throughout the year without variation in the muds used, thus making uniformity in the final product. The degree of drying is not sharply critical, however, in reference to the extraction process. Some moisture is desirable and moisture content as high as percent does not decrease the wax yield.

In the process of extracting the crude waxes to convert easily and simply from the muds, a number of organic solvents for.

the waxes may be used. Toluol, commonly known as toluene, has a number of advantages and is preferred. It is preferable to extract the wax at .a temperature somewhat above its melting point,

since this enhances its solubility. The solvent is recovered from the extracted residue. The crude wax solution will contain an insoluble sludge of finely divided mud particles which shouldvbe filtered out. The olvent is evaporated oil, but pref erably not entirely to completion, and recovered, and the crude wax, obtained as a residue still containing a proportion of solvent, is allowed to solidify either in blocks or in thin sheets. These can be chipped or broken into pieces so that they may be mixed with a selective solvent in the following described process:

The chipped or broken crude wax pieces are placed in a container and covered with a charge to separate the fatty of selective solvent (2. material which is an excellent fat solvent but which is a poor wax solvent). A number of solvents have been found suitable for this purpose, including acetone, ethyl methyl ketone, ethyl ether, petroleum and certain products, such as heptane, hexane, and those rich is pentanes. Acetone and methyl ethyl ketone are preferred to the other solvents because of their higher boiling points and less volatility and because of their tolerance toward moisture which may be a contaminant of the crude wax. The container may be closed to reduce solvent losses.

The fatty portions are separated from the crude wax by a process of diffusing into the solvent, which is preferably carried out at ordinary room temperatures of from 20 to 25 C. After standing about a day, the acetone solution (solvent containing the fatty portions) is drawn off and preferably a fresh supply of acetone is added. However, in the place of fresh acetone, an acetone solvent is recovered by distillation from both the wax residue and the fatty portion solution.

The wax residue, after beinggfreed from acetone, is melted and allowed to solidify. It is a hard and brittle wax product, ranging in color hard wax products thus obtained from clariflcation muds from raw sugar factories are shown below: i v

Saponiflcation values 27.2-53.3 Aci values 9.7-11.4 I e number (Hanus) 21.5-19.8

me sterols are present but not in detrimental quantities. Waxes of these characteristics are useful for industrial purposes. 7

The acetone soluble fatty portion contains valuable mixed fractions which are also recovered.

Such portion can be resolved without difliculty into three fractions: first, a crystalline product composed principally of sterols; second, a semisolid product composed acids; and third, a remaining residue.

The crystalline sterol fraction is recovered from a fairly concentrated solution of the fatty portion in acetone. This solution may be obtained by distilling only partof the acetone from the fatty portion solution remaining after separation of the hard lution is cooled to crystallize the sterols which are filtered off. The sterols thus obtained are purifled by recrystallization to obtain a stable mix wax. The concentrated soture. This fraction is a white or pale yellow crystalline mixture composed mainly of sterols. Such mixtures have been found to have melting points of 127- 142" C'., and specific rotation [1 values from? 32 to 44.3. Irradiation of said sterols by ultraviolet light yields a product having vitamin D potency.

After removal of the crystalline sterols, the I acetone is recovered by evaporation from the re,- maining solution, and the free fatty acid fraction is obtained from theresidue by subjecting it to an'alcohol extraction. This fraction is a brown semi-solid substance composed mainly of principally of free fatty fraction andthe free ble fraction from the fatty portion, the remaining residue fraction is a dark colored mass, semiwax into various constituents comprising mixing.

pieces of the crude wax with acetone and permitting the acetone to dissolve the fatty portions and not the hard wax constituents, separating the solution from the mixture and recovering the" hard wax constituents, on a. portion of the acetone from the solution to give a fairly con-' centrated solution, cooling the concentrated solution to crystallize a sterol fraction therein, and

separating and recovering the crystalline sterol ting the acetone to hard wax constituents,

fraction therefrom.

. 2. A method of separating crude sugar cane wax into various constituentscomprising mixing pieces of the crude wax with acetone and permitnot the hard wax solution from the mixture and recovering the distilling oif a portion of the acetone from the solution to give a fairly concentrated solution, cooling the concentrated so- I lution to crystallize a sterol fraction therein,sep-' arating and. recov the crystalline sterol fraction therefrom, evaporating the acetone from the remainingsolution, subjecting the residue'remaining after evapor tion of the acetone acid fraction. and recovering the residue remainto an alcohol extraction to recover a free fatty ing after extraction of the free fatty acid porfree fatty acids mixed with some sterols and 5 tion. t other minor constituents. ROYAL T. BALCH. After removal of both the crystalline sterol a cements of v tNo. 2381 420. August 7, 1.9-1.5. v ROYALT.BALCH It is hereby certified that error appears in the rinted specification of the above numbered patent requiring correction as follows: 36, strike out frotation [a',,"] values from 32 to age 2, first column, lines 35 and 44.33; and insert instead rotation lajgmluu of from 32 to -44.8.; and that the said Letters Patent should be read with correction therein in the Patent Ofice.

that the same may conform to the record of the case Signed and sealed out 19th day of March, A. D. 1 46.

' Commissioner qfPate'nts.

fatty acid or alcohol soluin fats. This fraction con-' dissolve the fatty portions and constituents, separating the hard wax products thus obtained from clariflcation muds from raw sugar factories are shown below: i v

Saponiflcation values 27.2-53.3 Aci values 9.7-11.4 I e number (Hanus) 21.5-19.8

me sterols are present but not in detrimental quantities. Waxes of these characteristics are useful for industrial purposes. 7

The acetone soluble fatty portion contains valuable mixed fractions which are also recovered.

Such portion can be resolved without difliculty into three fractions: first, a crystalline product composed principally of sterols; second, a semisolid product composed acids; and third, a remaining residue.

The crystalline sterol fraction is recovered from a fairly concentrated solution of the fatty portion in acetone. This solution may be obtained by distilling only partof the acetone from the fatty portion solution remaining after separation of the hard lution is cooled to crystallize the sterols which are filtered off. The sterols thus obtained are purifled by recrystallization to obtain a stable mix wax. The concentrated soture. This fraction is a white or pale yellow crystalline mixture composed mainly of sterols. Such mixtures have been found to have melting points of 127- 142" C'., and specific rotation [1 values from? 32 to 44.3. Irradiation of said sterols by ultraviolet light yields a product having vitamin D potency.

After removal of the crystalline sterols, the I acetone is recovered by evaporation from the re,- maining solution, and the free fatty acid fraction is obtained from theresidue by subjecting it to an'alcohol extraction. This fraction is a brown semi-solid substance composed mainly of principally of free fatty fraction andthe free ble fraction from the fatty portion, the remaining residue fraction is a dark colored mass, semiwax into various constituents comprising mixing.

pieces of the crude wax with acetone and permitting the acetone to dissolve the fatty portions and not the hard wax constituents, separating the solution from the mixture and recovering the" hard wax constituents, on a. portion of the acetone from the solution to give a fairly con-' centrated solution, cooling the concentrated solution to crystallize a sterol fraction therein, and

separating and recovering the crystalline sterol ting the acetone to hard wax constituents,

fraction therefrom.

. 2. A method of separating crude sugar cane wax into various constituentscomprising mixing pieces of the crude wax with acetone and permitnot the hard wax solution from the mixture and recovering the distilling oif a portion of the acetone from the solution to give a fairly concentrated solution, cooling the concentrated so- I lution to crystallize a sterol fraction therein,sep-' arating and. recov the crystalline sterol fraction therefrom, evaporating the acetone from the remainingsolution, subjecting the residue'remaining after evapor tion of the acetone acid fraction. and recovering the residue remainto an alcohol extraction to recover a free fatty ing after extraction of the free fatty acid porfree fatty acids mixed with some sterols and 5 tion. t other minor constituents. ROYAL T. BALCH. After removal of both the crystalline sterol a cements of v tNo. 2381 420. August 7, 1.9-1.5. v ROYALT.BALCH It is hereby certified that error appears in the rinted specification of the above numbered patent requiring correction as follows: 36, strike out frotation [a',,"] values from 32 to age 2, first column, lines 35 and 44.33; and insert instead rotation lajgmluu of from 32 to -44.8.; and that the said Letters Patent should be read with correction therein in the Patent Ofice.

that the same may conform to the record of the case Signed and sealed out 19th day of March, A. D. 1 46.

' Commissioner qfPate'nts.

fatty acid or alcohol soluin fats. This fraction con-' dissolve the fatty portions and constituents, separating the 

